| Summary: | Aluminum from saline slags generated during the recycling of this metal, extracted under reflux conditions with aqueous NaOH, was used in the synthesis of hydrocalumite-type solids with the formula Ca<sub>2</sub>Al<sub>1–m</sub>Fe<sub>m</sub>(OH)<sub>6</sub>Cl·2H<sub>2</sub>O. The characterization of the obtained solids was carried out by powder X-ray diffraction, infrared spectroscopy, thermal analysis, element chemical analysis, N<sub>2</sub> adsorption-desorption at −196 °C and electron microscopy. The results showed the formation of Layered Double Hydroxide-type compounds whose characteristics varied as the amount of incorporated Fe<sup>3+</sup> increased. These solids were calcined at 400 °C and evaluated for the catalytic photodegradation of ibuprofen, showing promising results in the elimination of this drug by advanced oxidation processes. The CaAl photocatalyst (without Fe) showed the best performance under UV light for the photodegradation of ibuprofen.
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